Process for making fullerene fibers

• US 5,591,312 A
• Filed: 05/15/1995
• Issued: 01/07/1997
• Est. Priority Date: 10/09/1992
• Status: Expired due to Term

• Current Assignee: Rice University
• Original Assignee: Rice University
• Inventors: Smalley, Richard E.
• Primary Examiner(s): Langel, Wayne
• Assistant Examiner(s): DI MAURO, PETER T
• Application Number:
  US08/441,432
• Time in Patent Office: 603 Days
• Field of Search: 423/445 B, 423/447.3, 423/DIG. 39, 423/DIG. 40, 204/157.47, 204/173, 204/157.41
• US Class Current: 204/157.41
• CPC Class Codes: D01F 9/12 Carbon filaments; Apparatus specially adapted for the manufacture thereof
• CPC Class Codes: Y10S 977/844 Growth by vaporization or dissociation of carbon source using a high-energy heat source, e.g. electric arc, laser, plasma, e-beam
• CPC Class Codes: Y10S 977/855 for manufacture of nanostructure

Abstract

This invention provides a method and apparatus for producing fullerene fibers by establishing an electric field between a needle electrode and an opposing electrode in the presence of carbon and a heat source. Carbon is directed by the electric field to the needle electrode and heated by the heat source to form a carbon-carbon bonded fullerene network. The needle electrode may be moved to lengthen the fullerene network into a fullerene fiber. Fullerene fibers of 0.5 cm or longer may be produced by this method.

Claims

1. A process for making a carbon fiber comprising one or more fullerene tubes, comprising:

(a) establishing an electric field between a needle tip and an opposing electrode;

(b) providing vaporized carbon to the space around the electric field to form a growing carbon-containing precursor for fullerene which precursor contains carbon-carbon bonds that have a fullerene structure on the needle tip;

(c) focusing a laser beam between the growing precursor and the opposing electrode; and

(d) withdrawing the needle tip from the opposing electrode while maintaining the electric field between the growing precursor and the opposing electrode and while providing vaporized carbon to the space around the electric field to form said carbon fiber.

2. A process in accordance with claim 1 wherein the needle tip and the growing precursor are electrically biased to ground.

3. A process in accordance with claim 2 wherein the electric field is maintained at a pressure of less than 0.001 Torr.

4. A process in accordance with claim 3 wherein the vaporized carbon is provided to the space around the electric field by introducing a carbon feedstock comprising paraffins, olefins, aromatics, alcohols, ethers, esters, aldehydes, ketones, alkynes or mixtures thereof to the space around the electric field.

5. A process in accordance with claim 4 wherein the carbon feedstock is anthracene.

6. A process in accordance with claim 3 wherein the vaporized carbon is provided to the space around the electric field by introducing a carbon feedstock comprising graphite to the space around the electric field.

7. A process in accordance with claim 3 wherein the vaporized carbon is provided to the space around the electric field by introducing a carbon feedstock comprising fullerenes to the space around the electric field.

8. A process in accordance with claim 7 wherein the carbon feedstock consists essentially of fullerenes.

9. A process in accordance with claim 8 wherein the fullerenes are selected from the group of (La@C₆₀), (La@C₈₂), (La₂ @C₆₆), (La₂ @C₈₈), (La₃ @C₉₄), (@C₆₀), (@C₇₀) and mixtures thereof.

10. A process in accordance with claim 3 wherein the carbon feedstock comprises boron or nitrogen.

11. A process for making carbon fibers comprising one or more fullerene tubes, which comprises:

(a) introducing carbon to a fiber growth site comprising an electric field and a laser beam for heating the growth site;

(b) guiding the carbon with the electric field to said growth site;

(c) reacting at least a portion of the carbon guided to the growth site into a carbon-containing precursor for fullerene which precursor contains carbon-carbon bonds that have a fullerene structure to form said carbon fiber; and

(d) maintaining the growth site positioned in the laser beam.

12. A process in accordance with claim 11, wherein the growth site is maintained positioned in the means for heating a growth site by manipulating the relative position of the fiber.

13. A process for making fullerene tubes comprising:

(a) providing a fullerene tube nucleation zone maintained in an electric field,

(b) providing a needle tip and a laser beam within the fullerene tube nucleation zone,

c) providing carbon to the fullerene tube nucleation zone under conditions sufficient to form a carbon-containing precursor for fullerene which precursor contains carbon-carbon bonds that have a fullerene structure, having a first end anchored to the needle tip and a second end open for bonding to additional carbon, and

(d) withdrawing the needle tip from the fullerene tube nucleation zone to maintain the second end within the laser beam in the fullerene tube nucleation zone.

14. A process for making a carbon fiber comprising one or more fullerene tubes, comprising:

(a) establishing an electric field between an initial fullerene growth site and an opposing electrode;

(b) focusing a laser beam between said initial fullerene growth site and the opposing electrode;

(c) providing vaporized carbon to a space around the electric field to form a growing carbon-containing precursor for fullerene which precursor contains carbon-carbon bonds that have a fullerene structure on said initial fullerene growth site; and

(d) withdrawing said initial fullerene growth site from the opposing electrode while maintaining the electric field between the growing precursor and the opposing electrode and while providing vaporized carbon to the space around the electric field to form said carbon fiber connected to said initial fullerene growth site.

15. A process in accordance with claim 14 wherein said initial fullerene growth site is a needle tip.

16. A process in accordance with claim 14 wherein said initial fullerene growth site is a carbon fiber.

17. A process in accordance with claim 14 wherein said laser beam is initially focused to heat said initial fullerene growth site and is maintained focused on the growing precursor as said initial fullerene growth site is withdrawn from the opposing electrode.

18. A process for making a carbon fiber comprising one or more fullerene tubes, comprising:

(a) establishing a high electric field having strength of 1 to 20 volts per Angstrom between a needle tip and an opposing electrode in the absence of an electrical discharge;

(b) providing vaporized carbon to the space around the high electric field to form a growing carbon-containing precursor for fullerene which precursor contains carbon-carbon bonds that have a fullerene structure on the needle tip; and

(c) withdrawing the needle tip from the opposing electrode while maintaining the high electric field between said growing precursor and the opposing electrode and while providing vaporized carbon to the space around the high electric field to form said carbon fiber.

19. A process in accordance with claim 18 wherein the needle tip and the growing precursor are electrically biased to ground.

20. A process in accordance with claim 19 wherein the high electric field is maintained at a pressure of less than 0.001 Torr.

21. A process in accordance with claim 20 wherein the vaporized carbon is provided to the space around the high electric field by introducing a carbon feedstock comprising paraffins, olefins, aromatics, alcohols, ethers, esters, aldehydes, ketones, alkynes or mixtures thereof to the space around the high electric field.

22. A process in accordance with claim 21 wherein the carbon feedstock is anthracene.

23. A process in accordance with claim 20 wherein the vaporized carbon is provided to the space around the high electric field by introducing a carbon feedstock comprising graphite to the space around the high electric field.

24. A process in accordance with claim 20 wherein the vaporized carbon is provided to the space around the high electric field by introducing a carbon feedstock comprising fullerenes to the space around the high electric field.

25. A process in accordance with claim 24 wherein the carbon feedstock consists essentially of fullerenes.

26. A process in accordance with claim 25 wherein the fullerenes are selected from the group of (La@C₆₀), (La@C₈₂), (La₂ @C₆₆), (La₂ @C₈₈), (La₃ @C₉₄), (@C₆₀), (@C₇₀) and mixtures thereof.

27. A process in accordance with claim 20 wherein the carbon feedstock comprises boron, nitrogen or mixtures thereof.

28. A process in accordance with claim 18 wherein a laser beam is focused between the growing precursor and the opposing electrode.

29. A process for making carbon fibers comprising one or more fullerene tubes, which comprises:

(a) introducing carbon to a carbon fiber growth site comprising an electric field having a field strength of 1 to 20 volts per Angstrom and a means for heating the growth site comprising a laser beam or light as the heat source;

(b) maintaining the electric field to prevent electrical discharges therein;

(c) guiding the carbon with the electric field to said growth site;

(d) reacting at least a portion of the carbon guided to the growth site into a carbon-containing precursor for fullerene which precursor contains carbon-carbon bonds that have a fullerene structure to form said carbon fiber; and

e) maintaining the growth site positioned in the means for heating said growth site.

30. A process in accordance with claim 29 wherein the growth site is maintained positioned in the means for heating a growth site by manipulating the relative position of the fiber.

31. A process in accordance with claim 29 wherein the means for heating a growth site is a laser beam.